TR201517742A2 - Fotopolimerizasyon Tekniği ile Altın Nanoparçacık İçeren Nanokompozit Filmlerin Hazırlanma Metodu - Google Patents
Fotopolimerizasyon Tekniği ile Altın Nanoparçacık İçeren Nanokompozit Filmlerin Hazırlanma Metodu Download PDFInfo
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- diacrylate
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 39
- 239000010931 gold Substances 0.000 title claims abstract description 38
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 32
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229920000642 polymer Polymers 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 21
- -1 poly(ethylene glycol) Polymers 0.000 claims description 17
- 239000000178 monomer Substances 0.000 claims description 12
- 125000004386 diacrylate group Chemical group 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 5
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 claims description 4
- GDOBGDUGIFUCJV-UHFFFAOYSA-N 2,2-dimethylbutane;2-methylprop-2-enoic acid Chemical compound CCC(C)(C)C.CC(=C)C(O)=O.CC(=C)C(O)=O.CC(=C)C(O)=O GDOBGDUGIFUCJV-UHFFFAOYSA-N 0.000 claims description 4
- OYKPJMYWPYIXGG-UHFFFAOYSA-N 2,2-dimethylbutane;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(C)(C)C OYKPJMYWPYIXGG-UHFFFAOYSA-N 0.000 claims description 4
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 4
- DOMLXBPXLNDFAB-UHFFFAOYSA-N ethoxyethane;methyl prop-2-enoate Chemical compound CCOCC.COC(=O)C=C DOMLXBPXLNDFAB-UHFFFAOYSA-N 0.000 claims description 4
- 229920001427 mPEG Polymers 0.000 claims description 4
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 claims description 4
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 4
- FSDNTQSJGHSJBG-UHFFFAOYSA-N piperidine-4-carbonitrile Chemical compound N#CC1CCNCC1 FSDNTQSJGHSJBG-UHFFFAOYSA-N 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- 229920002635 polyurethane Polymers 0.000 claims description 4
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 238000003848 UV Light-Curing Methods 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000000523 sample Substances 0.000 claims 1
- 238000009472 formulation Methods 0.000 description 19
- 238000004626 scanning electron microscopy Methods 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 229920006037 cross link polymer Polymers 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- QAOJPYQSRMWAMC-UHFFFAOYSA-N 2-sulfanylthioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(S)=CC=C3SC2=C1 QAOJPYQSRMWAMC-UHFFFAOYSA-N 0.000 description 3
- 229910004042 HAuCl4 Inorganic materials 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 150000003573 thiols Chemical class 0.000 description 3
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- SDKPSXWGRWWLKR-UHFFFAOYSA-M sodium;9,10-dioxoanthracene-1-sulfonate Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)[O-] SDKPSXWGRWWLKR-UHFFFAOYSA-M 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 150000003512 tertiary amines Chemical class 0.000 description 2
- LBDSQNRQXIKAGX-UHFFFAOYSA-N (2-methyl-3-prop-2-enoyloxypropyl) prop-2-enoate Chemical compound C=CC(=O)OCC(C)COC(=O)C=C LBDSQNRQXIKAGX-UHFFFAOYSA-N 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000412 dendrimer Substances 0.000 description 1
- 229920000736 dendritic polymer Polymers 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000022244 formylation Effects 0.000 description 1
- 238000006170 formylation reaction Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
-
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
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- C08F2/00—Processes of polymerisation
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- B82—NANOTECHNOLOGY
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- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
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- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
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Abstract
Fotopolimerizasyon Tekniği ile Altın Nanoparçacık İçeren Nanokompozit Filmlerin Hazırlanma Metodu Akrilik bazlı oligomer, akrilik bazlı monomer, tek bileşenli 2.tip radikalik bir fotobaşlatıcı olan 2-merkaptotiyokzanton ve kloroaurik asit içeren, altın ayna özelliğine sahip altın nanoparçacık içeren metal/polimer nanokompozit film ile ilgilidir. Şekil 1
Description
TARIFNAME
Fotopolimerizasyon Teknigi ile Altin Nanoparçacik Içeren Nanokompozit Filmlerin
Hazirlanma Metodu
Teknik Alan
Bulus, akrilik bazli oligomer, akrilik bazli monomer, tek bilesenli 2.tip radikalik bir fotobaslatici
olan 2-merkaptotiyokzant0n (1) ve kloroaurik asit içeren, altin ayna özelligine sahip altin
nanoparçacik içeren metal/polimer nanokompozit film ile ilgilidir.
Teknigin Bilinen Durumu
Konvensiyonel olarak, metal nanoparçaciklari, soy metallerin çesitli tuzlarinin çesitli
yöntemlerle indirgenmesi sayesinde sentezlenmektedir. Küresel formlu nanoparçaciklarin
geleneksel olarak sentezlenmesi için, sodyum sitrat ya da sodyum borohidrür ile indirgenme
islemi kullanilmaktadir. Bunun yaninda metal tuzlarinin UV isik ile fotoindirgenmesi bir diger
nanoparçacik elde etme yöntemidir.
Yüksek serbest yüzey enerjisinden ötürü, metal nanoparçaciklarin kolaylikla kümeleniyor
olmasi ve termodinamik açidan kararsiz parçaciklarin formülasyonda dagilmasi büyük bir
problemdir. Bu problemi asmak ve kararli parçaciklar elde etmek için çesitli yöntemler
kullanilmaktadir. Bunlara örnek olarak; sitrat indirgenmesi, tiyol stabilizasyon ve tiyoller,
aminler, miseller, dendrimer ve polimerlerin kullanildigi çesitli termal ve fotokimyasal teknikler
gösterilebilir.
Bilim dünyasinda Au nanoparçaciklarinin büyüklügü ve seklinin kontrolü büyük bir öneme
sahiptir. Çünkü belirli sekil ve büyüklük; optik, elektronik ve katalitik islemlerde önemlidir.
Ozellikle optik özellikleri parçacik sekline bagli oldugundan, Au nanoparçaciklarinin
kompozitlerde bulunmasi; biyo/nanotip, sensör, katalizör ve nanoteknoloji açisindan
önemlidir. Altin nanoparçaciklarin parçacik sekil ve boyutlari, UV-VIS spektrumlari
incelenerek tayin edilebilir ve yüzey plazmon bant etkisiyle 540 nm dalgaboyunda veya
parçacik boyutuna göre, daha az ya da daha fazla dalgaboyunda bir absorpsiyon gözlenir.
Benzer olarak gerçeklestirilen çalismalarda; formülasyonlara ilave olarak tersiyer amin
eklenerek olusacak olan oi-aminoalkil radikallerinin olumlu katkisi gözlenmistir.
Literatürdeki çalismalar incelendiginde (2-4); Polimer matriksinde nanoparçacik dagiliminin
SEM görüntüleri olusan nanoparçacik miktarinin, oldukça az oldugu ve hedeflenen ayna
görüntüsünün olusmadigi görülmüstür.
Mevcut teknikte yer alan çalismalarda, çesitli tip fotobaslaticilar ve bu baslaticilar,
beraberinde yardimci baslaticilar kullanilmistir. Yapilan bir çalismada; tiyokzanton
molekülünün uzun alkil zincirli tiyol türevleri fotobaslatici olarak, tersiyer aminler varliginda
kullanilmistir (3). Ve sonuç olarak da, tiyol etkisi net olarak gözlenememistir.
Sonuç olarak yukarida anlatilan yetersizliklerden dolayi, Au nanoparçacik içeren
nanokompozit filmlerin üretimi ile ilgili teknik alanda bir gelistirme yapilmasi gerekli
kilinmistir.
Bulusun Amaci
Mevcut bulus, yukarida bahsedilen gereksinimleri karsilayan, tüm dezavantajlari ortadan
kaldiran ve ilave bazi avantajlar getiren fotopolimerizasyon teknigi ile altin nanoparçacik
içeren nanokompozit filmlerin hazirlanma metodu ile ilgilidir.
Bulusun amaci, In-situ olarak iyonlarin nanoparçacik boyutuna çok kisa bir sürede ve boyut
ve dagilim kararliligi saglanarak minumum kümelesmeyle eldesidir. Metal/polimer nano
kompozit malzemede SEM görüntülerinden de görülecegi gibi dar bir boyut araliginda
kümelesme olmaksizin nanoparçacik olusumu ve bu parçaciklarin polimer matriksinde
dagilimi saglanmis ve ilk kez polimer matriks yüzeyinde biriken nanoparçaciklar yüzey
plasmaon etkisi sonucunda yansitici ayna görüntüsünün olusmasina yol açmistir.
Bulusun bir diger amaci, ihtiva ettigi nanoparçaciklarin tamamina yakininin küresel sekilde
olmasidir.
Bulusun bir benzer amaci, ihtiva ettigi nanoparçaciklarin boyutlarinin 30 ile 50 nm gibi dar bir
aralikta olmasidir.
Bulusun bir baska amaci, ihtiva ettigi nanoparçaciklarin, filmin yüzeyine, istiflenerek, gömülü
vaziyette olmasidir.
Bulusun bir diger amaci, elde edilen filmin, altin rengi ihtiva etmesidir.
Bulusun bir benzer amaci, çapraz bagli polimer olarak, poli(etilen glikol) diakrilat, poli(etilen
glikol) monoakrilat, poli(etilen glikol) metil eter akrilat, trimetilpropan triakrilat, dipropilen glikol
diakrilat, tripropilen glikol diakrilat, neopentil glikol diakrilat, 1,6-hekzanediol diakrilat, 2-metil-
1,3-propanediol diakrilat, neopentil glikol propoksilat(2) diakrilat, trimetilpropan trimetakrilat,
poliüretan akrilat veya epoksi akrilat kullanilmasidir.
Bulusun bir baska amaci, hem indirgeme, hem de polimerizasyon islemini gerçeklestirmek
üzere; fotobaslatici olarak, tek bilesenli 2.tip radikalik bir fotobaslatici olan 2-
merkaptotiyokzanton kullanilmasidir. Bu sayede; herhangi ikinci bir madde ilavesi
olmaksizin, molekuldeki tiyol grubunun, nanoparçacik stabilizasyonuna katkisi saptanmistir.
Ayrica tiyil radikalleri polimer matriksinin olusumuna katki saglarken olusan ketil radikalleride
iyonlarin nanoparçacik formuna indirgenmesine yardimci olmaktadir.
Bulusun bir diger amaci, altin tuzu olarak, kloroaurik asit (HAuCI4) bilesigi kullanilmasidir.
Bulusun bir benzer amaci, fotopolimerizasyon metodunun, in-situ olarak altin iyonlarinin
nanoparçaciklara indirgenmesini saglarken, bu nanoparçaciklarin içinde düzgün olarak
dagildigi çapraz bagli polimer matriksiri de olusmasini saglamasidir.
Yukarida anlatilan amaçlarin yerine getirilmesi için, altin ayna özelligine sahip altin
nanoparçacik içeren metal/polimer nanokompozit film olup, özelligi;
o akrilik bazli oligomer, akrilik bazli monomer, tek bilesenli 2.tip radikalik bir
fotobaslatici olan 2-merkaptotiy0kzanton ve kloroaurik asit ihtiva etmektedir.
Bulusun yapisal ve karakteristik özellikleri ve tüm avantajlari asagida verilen sekiller ve bu
sekillere atiflar yapilmak suretiyle yazilan detayli açiklama sayesinde daha net olarak
anlasilacaktir ve bu nedenle degerlendirmenin de bu sekiller ve detayli açiklama göz Önüne
alinarak yapilmasi gerekmektedir.
Bulusun Anlasilmasina Yardimci Olacak Sekiller
Sekil 1: Altin içeren ve altin içermeyen (F1) formülasyonun IR dönüsüm grafigidir.
Sekil 2: Altin içeren ve altin içermeyen polimerizasyon isi akisi grafigidir.
Sekil 3: Altin içeren ve altin içermeyen polimerizasyon hiz grafigidir.
Sekil 4: Altin içeren ve altin içermeyen polimerizasyon % dönüsüm grafigidir.
Sekil 5: Altin içeren F1A formülasyonunun farkli sürelerde UV isiga maruz kalmasiyla elde
edilen UV-VIS spektrumunun görünümüdür.
Sekil 6: Altin içeren F2A formülasyonunun farkli sürelerde UV isiga maruz kalmasiyla elde
edilen UV-VIS spektrumunun görünümüdür.
Sekil 7a: Altin içeren F1A formülasyonunun SEM (Taramali Elektron Mikroskobu) analizi
sonucu elde edilen 1 um görünümüdür.
Sekil 7b: Altin içeren F1A formülasyonunun SEM (Taramali Elektron Mikroskobu) analizi
sonucu elde edilen 500 nm görünümüdür.
Sekil 7c: Altin içeren F1A formülasyonunun SEM (Taramali Elektron Mikroskobu) analizi
sonucu elde edilen 200 nm görünümüdür.
Sekil 7d: Altin içeren F1A formülasyonunun SEM (Taramali Elektron Mikroskobu) analizi
sonucu elde edilen kesit görünümüdür.
Çizimlerin mutlaka ölçeklendirilmesi gerekmemektedir ve mevcut bulusu anlamak için gerekli
olmayan detaylar ihmal edilmis olabilmektedir. Bundan baska, en azindan büyük ölçüde
özdes olan veya en azindan büyük ölçüde özdes islevleri olan elemanlar, ayni numara ile
gösterilmektedir.
Kisaltmalar:
F1: Altin içermeyen
F1A- F2A: Altin içeren
Bulusun Detayli Açiklamasi
Bu detayli açiklamada, bulus konusu fotopolimerizasyon teknigi ile altin nanoparçacik içeren
nanokompozit filmlerin hazirlanma metodunun tercih edilen yapilanmalari, sadece konunun
daha iyi anlasilmasina yönelik olarak ve hiçbir sinirlayici etki olusturmayacak sekilde
açiklanmaktadir.
Bulus, altin ayna özelligine sahip altin nanoparçacik içeren metal/polimer nanokompozit film
hazirlama metodudur. Söz konusu yöntemde; hem indirgeme, hem de polimerizasyon
islemini gerçeklestirmek üzere; çok fonksiyonlu akrilat ve seyreltici monomer; tek bilesenli
2.tip radikalik bir fotobaslatici olan 2-merkaptotiy0kzanton; altin tuzu olarak ise, kloroaurik
asit (HAuCI4) bilesigi kullanilmaktadir. Bunlara ek olarak, nanokompozitlerin oda sicakliginda,
hizli ve etkin olarak üretilmesi için; çapraz bagli polimer matriks olusturulmasi ve iyonlarin in-
situ olarak altin nanoparçaciklara indirgenmesi fotopolimerizasyon metodu ile
gerçeklestirilmektedir.
Bulus konusu üretim metodu, asagidaki formülasyonu içermektedir. Söz konusu
formülasvon, degisik oranlarda kullanilan 2-Merkapt0tiv0kzanton ile 2 adettir.
Form'i'ilasyon HAuCI4 2-Merkaptotiyokzanton
Oligomer Monomer
Bahsedilen form'ulasyonda çapraz bagli polimeri hazirlamak için, akrilik bazli Oligomer ve
akrilik bazli monomer olarak; poli(etilen glikol) diakrilati poli(etilen glikol) monoakrilat,
poli(etilen glikol) metil eter akrilat, trimetilpropan triakrilat, dipropilen glikol diakrilat, tripropilen
glikol diakrilat, neopentil glikol diakrilat, 1,6-hekzanedi0l diakrilat, 2-metil-1,3-propanedi0l
diakrilat, neopentil glikol propoksilat(2) diakrilat, trimetilpropan trimetakrilat, poliüretan akrilat
veya epoksi akrilat kullanilmaktadir.
Istenilen formlßsvongaki oranlar kullanilarak, alt_in nanomrçacik içeren
nanokompozit film hazirlama metodu;
1) Formülasvon kullanilarak solüsyon hazirlanmasi:
2-Merkaptotiyokzanton ve; HAuCI4 'L'in, oda sicakliginda beher içerisine koyulmasi,
o akrilik bazli Oligomer ve monomerin ilavesi,
. elde edilen akrilik bazli karisimin, yaklasik 15 dakika süre ile oda sicakligindaki
ultrasonik banyoya birakilmasi,
o ardindan, prob tipli ultrasonik karistirici vasitasiyla, yaklasik 2 saniye karistirilarak,
homojen hale getirilmesi,
o son olarak, ultrasonik banyo ile degas edilmesi,
2) Solüsvon vasitasiyla. nanokompozit film eldesi:
o elde edilen solüsyonun, cam plaka üzerine, 40 mikrometre kalinlikta olacak sekilde
kaplanmasi,
o UV-kürlestirme cihazi vasitasiyla, UV isigina maruz kalmasidir.
SH UV Isik C 8
n | _-> Çapraz Bagli Polimer
Deneysel Çalismalar:
Bulus konusu formülasyon sentezlendikten sonra FTIR (Fourier Transform Infrared)
spektrumlarindan yararlanilarak, bulusun eldesine yönelik verim hesaplandi.
Formülasyonlarin belirli sürelerde isiga maruz birakilmasi sonucu FTIR spektrumlari alindi
ve 164Ocm45de ki pikte görülen azalma kaydedildi. Yüzde dönüsüm hesaplandi. (Sekil 1).
Beklenildigi gibi Au tuzu içeren formülasyonlarin dönüsüm yüzdeleri daha düsük olarak elde
edildi.
Polimerizasyon isi akisi (Sekil 2), hiz (Sekil 3), yüzde dönüsüm (Sekil 4) grafigi, ayrica Foto-
DSC (Diferansiyel Taramali Kalorimetre) çalismasi ile incelendi. Burada inert ortamda Au
nanoparçacik içeren formülasyonun dönüsüm yüzdesinin daha fazla oldugu görüldü.
Nanokompozit malzeme içerisindeki altin nanoparçaciklarin karakterizasyonu için ise, UV-
VlS spektrumlarindan faydalanildi (Sekil 5,6 ve 7). Spektrum incelendiginde; 510-570
arasinda absorpsiyon yapmistir.
Literatürde de var oldugu gibi Au nanoparçaciklarin olusumu ispat edilmistir. Absorpsiyon
araligi bize nanoparçacik boyutunun dar bir aralikta olustugunu göstermektedir.
SEM diyagrami incelendiginde ise; 1 numarali formülasyonda elde edilen nanopartiküller
görülmektedir. Nanopartiküller agirlikla küresel sekilde olup, 30-40 nm çapa sahiptirler. 1
numarali formülasyon için; Sekil ?arda 1 um; Sekil 7b'de, 500 nm; Sekil Tc>de, 200 nm; Sekil
7dide, kesit görünümü bulunmaktadir.
SEM grafikleride UV-Vis sonuçlarini dogrulamistir. Nanoparçacik boyut kararliligi ve
nanoparçaciklarin dagiliminin düzenli ve çok az kümelesmenin oldugunu göstermektedir.
Claims (8)
1. Altin ayna özelligine sahip altin nanoparçacik içeren metal/polimer nanokompozit film olug, özelligi; o akrilik bazli oligomer, akrilik bazli monomer, tek bilesenli 2.tip radikalik bir fotobaslatici olan 2-merkaptotiyokzanton ve kloroaurik asit içermesidir.
2. Istem 1'e uygun nanokompozit film olup, özelligi; akrilik bazli oligomer ve akrilik bazli monomer olarak; poli(etilen glikol) diakrilat, poli(etilen glikol) monoakrilat, poli(etilen glikol) metil eter akrilat, trimetilpropan triakrilat, dipropilen glikol diakrilat, tripropilen glikol diakrilat, neopentil glikol diakrilat, 1,6-hekzanediol diakrilat, 2-metiI-1,3-pr0panediol diakrilat, neopentil glikol propoksilat(2) diakrilat, trimetilpropan trimetakrilat, polii'iretan akrilat veya epoksi akrilat içermesidir.
3. istem 1ie uygun nanokompozit film olup, özelligi; %76,4wt akrilik bazli oligomer, %19,1 wt akrilik bazli monomer, %0,5 wt 2-merkapt0tiyokzant0n, %4 wt kloroaurik asit içermesidir.
4. istem 1'e uygun nanokompozit film olup, özelligi; %76 akrilik bazli oligomer, %19 wt akrilik bazli monomer, %1 wt 2-merkaptotiyokzanton, %4 wt kloroaurik asit içermesidir.
5. Altin ayna özelligine sahip altin nanoparçacik içeren metal/polimer nanokompozit film a) tek bilesenli 2.tip radikalik bir fotobaslatici olan 2-merkaptotiyokzanton ve kloroaurik asitin, oda sicakliginda bir beher içerisine koyulmasi, b) ardindan, akrilik bazli oligomer ve monomer ilavesi, c) elde edilen akrilik bazli karisimin, yaklasik 15 dakika süre ile, oda sicakligindaki ultrasonik banyoya birakilmasi; ve, bir karistirici vasitasiyla karistirilarak, homojen hale getirilmesi, d) ardindan da, ultrasonik banyo ile degas edilmesi, islem adimlari ile elde edilen solüsyonun, e) cam plaka üzerine kaplanmasi, f) UV-k'ürlestirme Cihazi vasitasiyla, UV isigina maruz kalmasi islem adimlarini içermesidir.
6. istem 5'e uygun üretim metodu olup, özelligi; c islem adiminda bahsedilen karistirma isleminin, prob tipli ultrasonik bir karistirici vasitasiyla yapilmasidir.
7. Istem 5'e uygun 'üretim metodu olup, özelligi; c islem adiminda bahsedilen karistirma isleminin yaklasik 2 saniye yapilmasidir.
8. istem 55e uygun 'üretim metodu olup, özelligi; akrilik bazli oligomer ve akrilik bazli monomer olarak; poli(etilen glikol) diakrilat, poli(etilen glikol) monoakrilat, poli(etilen glikol) metil eter akrilat, trimetilpropan triakrilat, dipropilen glikol diakrilat, tripropilen glikol diakrilat, neopentil glikol diakrilat, 1,6-hekzanediol diakrilat, 2-metiI-1,3-pr0panediol diakrilat, neopentil glikol propoksilat(2) diakrilat, trimetilpropan trimetakrilat, poli'üretan akrilat veya epoksi akrilat içermesidir.
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US16/067,118 US10526240B2 (en) | 2015-12-31 | 2016-12-28 | Preparation method of nanocomposite films comprising gold nanopoarticle via photopolymerization technique |
DE112016006130.7T DE112016006130T5 (de) | 2015-12-31 | 2016-12-28 | Verfahren zur Herstellung von Nanokompositfilmen, die Goldnanoteilchen umfassen, durch ein Photopolymerisationsverfahren |
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